Process of dehydrating moist chlorin.



E. A SPERRY. I PROCESS OF DEHYDRATING MOIST GHLOBIN.

APPLICATION FILED 0OT.4, 1907.

. Patented, Dec. 1, 1908.

Alf/army's UNITED srna ns PATENT OFFICE.

ELMER A. SPER RY, OF BROOKLYN, NEW YORK.

Specification of Letters Patent.

PROCESS OF DEHYDBATING MOIST CHLORIN.

Patened Dec. 1, 1908.

Application filed October 4, 1907. Serial No. 395,866.

specification.

ess which will My invention relates to the method of drying chlorin orrendering same anhydrous. The raw material is supposedto be gaseouschlorin either pure or diluted, as, for instance, by moisture or byother gases or vapors.

The process consists in various steps and operations calculated to bringabout the desired result.

To illustrate one form of apparatus with which the process may becarried out the accompanying drawings have been prepared in whichsimilar characters of reference indicate like parts throughout.

Figure 1, of the drawings, represents a diagrammatic view of theapparatus. Fig. 2, represents the same view with a part of the unitsdifferently coupled.

Generally speaking chlorin is extremely difficult to dry and especiallyto render absolutely anhydrous. I have found that a v 'ry pragticalmethod for accomplishing the ject is" to refrigerate, but when this isacpom'plished the chambers where refrigerai'on takes place may becomeclogged with the solid hydrate produced and the prc-css is thusinterrupted. 1 have provided means whereby this difficulty is overcomeand also whereby a number of desirable objects are attained inconnection with the pro-chilling of the gas; also heat exchange betweenthe incoming gas and product, and also recoven ing all the chlorin fromthe water and products to prevent waste of chlorin and also to preventany obnoxious odors in and about the plant which would otherwiseinevitably occur.

It is well known that an atmosphere containin one three millionth partchlorin is not sultable for breathing for any length of time, thus it isimportant to provide a procprevent escape of chlorin during operation.

Suppose chlorin to enter the apparatus at 3, from any suitable source ofsupply, for instance, electrolytic cells decomposing chlorids. The gasis preferably first led to a tower 4, or scrubber, through which it' maypass in an upward direction, and from which it passes through pipe 5;encountering in its upward passage a downwardly flowing stream of asuitable refrigerant, for instance, wate coming from the refrigerator somarked to the top of the tower 4, by pipe 6, and out at the bottom,returning to the refrigerator by pipe 7. From pipe 5, the

chlorin passes to chamber 8, thence to chamher 9, and through this tochamber 10 by pipes 12. After it has left chamber 10, the pipe 13carries the dried chlorin to any suitable reaction or other apparatus,as X, to the suction fan, or equivalent apparatus 14. The chamber 11 hasits jacket coupled to that of the chamber which is first in series, viz.chamber 8, by pipe 15 and in this particular instance the chamber 11 iswarming up, receiving its heat from the incoming gases as they passchamber 8 by means of the fluid jacket circulation. By this operationchlorin hydrate is accumulated in each of the chambers 10, 9 and 8 inthis order, which is in inverse ratio to the temperatures; thesetemperatures may be inferredby the temperature viz: minus 20 C. markedon the pipes 16 and 0 C. on the pipe 17 and 5 C. on pipe 18respectively, connecting the refrigerator with the jackets of thevarious chambers, as will readily be understood. This is true where theseries relation of the chainhers is used but it is not important toessential features of my invention that this arrangementbe alwaysemployed. 1

.It will furthermore be noticed that the refrigeration received by thegases in chanr her 8 is derived from the idle chamber 11. A receptacle10 is shown as receiving the liquid discharge from the idle chamber. InFig. 1 the idle chamber is coupled for discharge of the chlorin into thepipe 5 by pipe 20, whereupon it will be noted that the chlorin thusproduced is again refrigerated to remove any remaining moisture. In Fig.2 this pipe 20 is shown in dotted lines only and the melting of thehydrate is utilized to produce the two component liquids, chlorin andwater, the water being eliminated or drawn off in receptacle 19 and thechlorin collected and utilized as liquid chlorin in either the idlevessel or transferred to'othcr rece taclcs before 118111 The water drawnreceive heat to decompose the hydrate into 3 through duct 22, which as:will be seem? places the chamber 21 under negative pres sure ofexhauster 14:.

Referring now to Fig. 2, it will be seen thatthe process is carried outin identically the same manner as in Fig. l, but that the chamber 10 hasbecome so filled with the hydrate that a change is necessary. At thesame time chamber 11, which in Fig. l was idle, has now become the firstin the series and coupled with the inlet pipe 5; chamber 10 becoming theidle chamber, should now the original chlorin and water so as toeliminate the latter. In this arrangement it will be noticed thatchamber 9 has become the last of the series, which is always the'coldcstchamber, and will be next in order of rotation in the series to becomeidle. and pass through the process of having its accumulation of hydratetreated.

From the location and connection of the tan, or equivalent exhaustingapparatus let, it is apparent that the whole connected system duringoperation may be kept at av reduced atmospheric or negative pressure, sothat if any of the apparatus springs a leak the chlorin will not flowfrom the apparatus outwardly; but from the fact that the ap paratusisinhalent, air will flow into the apparatus but no chlorin escape. Theproportion of the chlorin which is converted into the hydrate may beregulated by the amount of moisture permitted to enter the system andtherefore the chambers; as from boiler 21. It willthus be seen that all,or nearly all, of the chlorin may be thus con verted if desired.

The chamber 10, in Fig. 2, it not coupled to the circuit as by the duct,shown in dotted lines at 20, will be found to be under positive pressureafter sui'iicient heat has been supplied for melting the chlorinhydrate.

The use and operation of the apparatus has been carefully pointed out inits description and needs no further amplification to aid in the properoperation and manipulation of the system by those versed in the art towhich it appcrtains. It will readily be understood that some of thesteps may be omitted or altered and equivalents may be substitut d, andthe invention extends to such use.

1 claim:

1; The process of dehydrating moist chlorin which consists inrefrigerating the gas in a plurality of chambers, thereby producingchlorin hyd'ate in such chambers, disconnecting a part of such chambersfrom the system and treating the contents of such disconnected chambersfor the separation of chlorin and Water.

'2. The process of dehydrating moist chlorin gas contained in a mixtureof chlorin and other gas or gases or vapor, which consists inrefrigerating the gas while in transit through a suitable chamber,thereby forming chlorin hydrate from the chlorin content of such gas andremoving the other gas or gases from the chamber.

3. The process oft dehydrating moist chlorin which consists inrefrigerating the gas in a plurality of chambers, thereby producingchlorin. hydrate in such chambers, disconnecting a part of such chambersfrom the system and treating the contents of such disconnected chambersfor the liquefaction of the hydrate and the separation of the chlorinand water.

l. The process of dehydrating moist chlorin which consists inrefrigerating the gas in a plurality of chambers coupled in a series,thereby producing chlorin hydrate in such chambers, disconnecting a partof such chambers from the series and treating the contents of suchdisconnected chambers for the separation of chlorin and Water.

5. The process of dehydrating moist chlorin gas contained in a mixtureof chlorin and other or gases or vapor, which consists in refrigeratingthe gas while in transit through a suitable chamber, thereby formingchlorin hydrate from the chlorin content of such gas and such moistureas is present andremoving the other gas or gases together with thegaseous chlorin not so converted from the chambers.

6. The process of dehydrating moist chlo-" rin which consists inrefrigeratin the gas;

in a plurality of chambers couple in a. se-

ries, thereby producing chlorin hydrate inf such chambers, chambers fromthe series disconnecting a part pf such and treatingthe contents of suchdisconnected chambers by; heat abstracted from the incoming chlorin" forthe separation of chlorin and water. 7. The'process of dehydrating moistgaseous chlorin which consists in adding moisture to the gas,refrigerating the gas in a plurality of chambers coupled in a series,

thereby producing chlorin hydrate in such chambers, disconnecting a partof such cham hers from such series and treating the contents of suchdisconnected chambers for the separation of chlorin and Water.

8. The process of dehydrating moist chlorin which consists inrefrigerating the gas in "a suitable chamber or chambers, therebyforming chlorin hydrate in a part of such chambers, treating thecontents oi'the chamber or chambers for the separation of chlorin andwater and further separating chlorin from the water thus obtained, underconditions of pressure below that of the surrounding atmosphere, for thepurposes specified.

9. The process of dchydri ting molst chlorin which consists inrefrigerating the gas in a plurality of chambers, thereby produccomesing chlorin hydrate in such chn nbersi, disconnecting a part of suchchambers from the system, and treating the contents of such of suchchambers from the system and treat ing the contents of such disconnectedchainbersfor the separation of chlorin and W stein 11. The process ofdehydrating moist chlorin Which consists in first chilling the gas bythe Wet contact process and then refrigerating seine in n plurality ofchambers,

thereby producing chlorin hydrate in such chambers, disconnecting itpart oi such chenibers from the system and treating the con tents ofsuch disconnected chambers for the 'rin hydrate in such chambers, therefrigeration in one or more of such chambers tit being produced by themelting chlorin hydrztte in another or others ofthe group.

it. The process of dehydrating moist chlorin gas contained in a mixtureof chlogin and other or gases or vapor, which con sists in refrigeratingthe gas While in transit through a suitable chamber, thereby form ingchlorin hydrate from the chlorin content ot' such gas and removing theother gas or irom the chamber under pressure below that of thesurrounding atmosphere.

if). The process of dchydrn g moist rhlorin whim consists in convcrtingg chlorin intochlorin hydrate by refrigeration, decomposing the hydrateinto chiorin gas and Water purpose specified.

1b. The process of. dehydrating moist chlorin which consists inconverting chlorin into chlorin hydrate by rei'frigerzition decomposingthe hydrate into chlorin gas and Water, and refrigerating the gas soproduced down to a point below that at which chlorin hydrate isproduced; y

17. The process of dehydrating moist, gaseous chlorin, which consists inadding moisture-to the gas, refrigerating the gels in a suitable chamberto a point at or below that at "which chlorin hydrate is formed, andtreating the contents of the cl'inmber to effect. decomposition of theproduct.

In'testimony whereof I have hereunto set my hend in presence of twosubscribing witnesses.

and rechilling the as so produced for the ELMER A. SPERRY.

